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Catalyst for preparing cyclohexanone by phenol hydrogenation and preparation method thereof

A technology for catalyst and hydrogen preparation, which is applied in catalyst activation/preparation, molecular sieve catalysts, chemical instruments and methods, etc. It can solve the problems of easy loss of precious metals, poor cycle stability, high consumption of precious metals, etc., and achieve high catalytic intrinsic activity and low cost , the effect of uniform dispersion of metal particles

Active Publication Date: 2020-03-24
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In contrast, solid Lewis acid can replace liquid Lewis acid as a reaction catalyst for phenol hydrogenation, effectively solving the problem of catalyst and product separation, but solid Lewis acid catalyst has disadvantages such as low catalytic efficiency, expensive carrier, and high amount of noble metal (active metal palladium Relatively high proportion of phenol)
In addition, the specific surface area of ​​conventional solid Lewis acid carriers is low, the precious metals are easily lost, and the cycle stability is poor.

Method used

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  • Catalyst for preparing cyclohexanone by phenol hydrogenation and preparation method thereof
  • Catalyst for preparing cyclohexanone by phenol hydrogenation and preparation method thereof
  • Catalyst for preparing cyclohexanone by phenol hydrogenation and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A kind of phenol hydrogenation prepares cyclohexanone catalyst and preparation method thereof, comprises the steps:

[0029] Preparation of the carrier: Under stirring conditions, weigh 15 g of industrial grade H-Beta molecular sieve, 500 g of concentrated nitric acid, and 150 g of distilled water, and mix them evenly. and ZrOCl 2 ·8H 2 O0.16 g and 15 g of distilled water were mixed evenly, mixed in a hydrothermal kettle at 80 °C for 24 h, filtered and dried with suction; the obtained product was roasted in an air atmosphere at 550 °C for 4 h to obtain a carrier.

[0030] Catalyst preparation:

[0031] 0.0168 g PdCl 2 Dissolve in hydrochloric acid solution, add 10 mL of distilled water; weigh 1 g of the above carrier in a 50 mL beaker, add 20 mL of distilled water. After the two were mixed evenly, they were stirred at room temperature for 2 h. Rotary steam at 50°C, then put it in a hydrogenation furnace for activation, the activation condition is: 10% H 2 / Ar, the...

Embodiment 2

[0034] A kind of phenol hydrogenation prepares cyclohexanone catalyst and preparation method thereof, comprises the steps:

[0035] Preparation of the carrier:

[0036] Under stirring conditions, weigh 15 g of industrial-grade H-Beta molecular sieve, 500 g of concentrated sulfuric acid, and 50 g of distilled water and mix evenly. Reflux for 15 h in an oil bath at 105°C and cool to room temperature to obtain the product; mix the above product with ZrOCl2 ·8H 2 O 0.16 g and 15 g of distilled water were mixed evenly, mixed in a hydrothermal kettle at 80 °C for 6 h, and the obtained product was calcined in an oxygen atmosphere at 550 °C for 4 h to obtain a carrier.

[0037] Catalyst preparation:

[0038] 0.0168 g PdCl 2 Dissolve in hydrochloric acid solution, add 10 mL of distilled water; weigh 1 g of the above carrier in a 50 mL beaker, add 20 mL of distilled water. After the two were mixed evenly, they were stirred at room temperature for 2 h. Rotary steam at 50°C, then put...

Embodiment 3

[0040] A kind of phenol hydrogenation prepares cyclohexanone catalyst and preparation method thereof, comprises the steps:

[0041] Preparation of the carrier:

[0042] Under the condition of stirring, 15 g of industrial-grade H-Beta molecular sieves, 500 g of concentrated sulfuric acid, and 150 g of distilled water were mixed evenly. Reflux for 15 h in an oil bath at 105°C and cool to room temperature to obtain the product; mix the above product with ZrOCl 2 ·8H 2 O 0.16 g and 15 g of distilled water were mixed evenly, treated in a hydrothermal kettle at 180°C for 24 h, filtered and dried by suction; the obtained product was roasted at 550°C for 4 h in a nitrogen atmosphere to obtain a carrier.

[0043] Catalyst preparation:

[0044] 0.0168 g PdCl 2 Dissolve in hydrochloric acid solution, add 20 mL of distilled water; weigh 1 g of the above carrier in a 50 mL beaker, add 20 mL of distilled water. After the two were mixed evenly, they were stirred at room temperature for ...

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Abstract

The invention discloses a catalyst for preparing cyclohexanone by phenol hydrogenation and a preparation method thereof. The method comprises the following steps: (1) acid is quickly mixed with a Betamolecular sieve, reflux treatment is carried out, centrifugal filtering is carried out after the reaction is finished, Zr salt or Sn salt is mixed with a reaction product, and the mixture is filtered, dried and roasted to obtain an activated strong Lewis solid acid material which has at least one pore size distribution at 1-10nm and certain alkalinity; and (2) Pd salt is prepared into a solution,and the solution is added into the material to obtain the catalyst which has high specific surface area, strong L acid and high metal dispersity. The catalyst provided by the invention is low in cost, simple in preparation method and high in catalytic activity. The turnover frequency (TOF) is higher than 100h<-1>. The phenol conversion rate and the cyclohexanone selectivity can reach 99% or above. Good stability is still shown after a cyclic test. The reaction product and the catalyst are easy to separate.

Description

technical field [0001] The invention relates to a catalyst for preparing cyclohexanone by hydrogenation of phenol and a preparation method thereof, belonging to the technical field of catalyst preparation. Background technique [0002] Phenol (C 6 h 5 OH) is a colorless needle-like crystal with a special smell, which is toxic and is an important organic chemical raw material, and is an important raw material for the production of phenolic resins, fungicides, preservatives and drugs (such as aspirin). Phenol exists in coal tar, so coal tar is one of the industrial sources of phenol. [0003] The phenol method is the earliest method for industrial production of cyclohexanone. It has the advantages of less side reactions, simple product separation and purification process, and high product purity. It is divided into gas-phase method and liquid-phase method. The gas-phase hydrogenation method usually uses 3 to 5 reactors in series, with supported Pd as the catalyst. This proc...

Claims

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Application Information

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IPC IPC(8): B01J29/74B01J37/10B01J37/02B01J35/10C07C45/00C07C49/403
CPCC07C45/006B01J29/7415B01J37/10B01J37/0201C07C2601/14B01J2229/18B01J35/618B01J35/615B01J35/617B01J35/643B01J35/647C07C49/403Y02P20/52
Inventor 涂椿滟刘昌伟陈奇毋肖卓李文林黄伟
Owner TAIYUAN UNIV OF TECH
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